CN113462389A - Thermochromic fluorescent temperature measuring material and preparation method and application thereof - Google Patents
Thermochromic fluorescent temperature measuring material and preparation method and application thereof Download PDFInfo
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- CN113462389A CN113462389A CN202110704884.9A CN202110704884A CN113462389A CN 113462389 A CN113462389 A CN 113462389A CN 202110704884 A CN202110704884 A CN 202110704884A CN 113462389 A CN113462389 A CN 113462389A
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Abstract
The invention provides a thermochromic fluorescent temperature measuring material and a preparation method and application thereof. The chemical general formula of the fluorescent temperature measuring material is YNbO4：x Bi3+‑y Eu3+，YNbO4As doping ions Bi3+‑Eu3+Of a transition metal Bi3+The introduction of the material effectively solves the problem of low sensitivity of a single luminescence center, and the material can change color with naked eyes when being heated to reach 473K (200 ℃) within ultraviolet light, changes from purple to pink and finally to red, and can directly measure the temperature. The preparation method adopts a solid phase method, is simple to operate, has low requirements on equipment and low production cost, and the prepared material has high purity, better optical performance and stable physicochemical properties. Fluorescence according to the inventionThe temperature measuring material has the advantages of convenient temperature measurement and great advantage. The invention also provides a standard colorimetric card temperature measurement technology, realizes low-cost temperature detection, and provides a new application technology for the optical thermometer.
Description
Technical Field
The invention relates to the technical field of application of down-conversion luminescent materials, in particular to a thermochromic fluorescent temperature measuring material and a preparation method and application thereof.
Background
Accurate and fast temperature measurement is crucial for scientific research and industrial production. The traditional radiation thermometry method has the advantages of wide working temperature range, fast response to temperature change, electromagnetic field interference resistance and the like, and can meet the requirement of accurate thermometry. However, the temperature measurement accuracy is degraded due to sensitivity to stray light, reflected light and flame disturbance during the temperature measurement process.
Non-contact optical thermometers based on temperature dependent phosphor materials are of interest for their fast response, low risk and excellent spatial resolution. The method has the advantages of radiation temperature measurement and overcomes a part of the defects of the radiation temperature measurement, and is a novel temperature measurement method. The single-emission optical thermometer has certain limitations in practical use due to the influence of light radiation and sample size fluctuation. At present, most researches are carried out on realizing temperature detection by utilizing up-conversion luminescence of a thermal coupling energy level of rare earth ions. However, most of the fluorescent thermometric materials with up-conversion luminescence have low temperature sensitivity, and due to the narrow thermal coupling energy level, the thermochromic thermometric materials have no thermochromic performance and low spatial resolution.
Disclosure of Invention
The invention aims to provide a thermochromic fluorescent temperature measuring material and a preparation method and application thereof, aiming at the defects in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a fluorescent temperature measuring material, which is Bi3+-Eu3+Doping YNbO4The chemical formula is YNbO4：x Bi3+-y Eu3+Wherein x is more than or equal to 0.005 and less than or equal to 0.02; y is more than or equal to 0.002 and less than or equal to 0.03, and x represents Bi3+Substituted Y3+The molar content of (a); y represents Eu3+Substituted Y3+The molar content of (a).
Furthermore, the ratio x to y of x to y is in the range of 0.25-6.
The invention also provides a preparation method of the thermochromic fluorescent temperature measuring material, which comprises the following steps:
step S1, according to the chemical formula YNbO 4: x Bi3+-y Eu3+Weighing solid compounds containing Y, Nb, Bi and Eu elements according to the stoichiometric ratio of the elements, and putting the solid compounds into a mortar for uniform grinding to obtain a mixture;
step S2, placing the mixture into a high-temperature tube furnace, and sintering for 2-6 hours at 1200-1500 ℃ in an air environment;
and step S3, taking the mixture out of the tube furnace after the mixture is cooled, and grinding the mixture into powder again to obtain the fluorescent temperature measuring material.
Further, in step S1, the solid compound is one or more of oxides, carbonates, or nitrates containing Y, Nb, Bi, and Eu elements.
Further, in step S2, the sintering temperature is 1250-1400 ℃.
Further, the sintering time is 3-5 hours.
The invention also provides application of the fluorescence temperature measurement material, and the fluorescence temperature measurement material is applied to a standard colorimetric card temperature measurement technology.
Furthermore, the temperature measurement range of the standard colorimetric card temperature measurement technology is 298K-473K.
The technical scheme provided by the invention has the beneficial effects that:
(1) YNbO is utilized as the fluorescent temperature measuring material4As doping ions Bi3+-Eu3+Substrate of (1), Compound YNbO prepared4：x Bi3+-y Eu3+High purity, good optical performance and stable physicochemical property, solves the problem of low sensitivity of a single luminescence center, and introduces Bi into the same matrix in the form of a combined pair of transition metal and rare earth ion3+-Eu3+The fluorescent temperature measuring material with high sensitivity of 1.63% is developed by utilizing the different luminescent colors and temperature quenching characteristics of the two luminescent centers, and theoretical guidance is provided for the combination based on the transition metal-rare earth ion type later. The fluorescent temperature measuring material of the invention is excited by ultraviolet light and is within 473K (200 ℃),the phenomenon that the fluorescence temperature measuring material changes color when being heated can be seen by naked eyes, the color changes from purple to pink and finally to red, the obvious color change enables people to directly measure the temperature, and compared with other fluorescence temperature measuring materials needing a professional spectrometer to measure the temperature, the fluorescence temperature measuring material has the advantages of convenient temperature measurement and great superiority;
(2) the preparation method of the fluorescence temperature measuring material provided by the invention adopts a solid phase method for synthesis, is prepared by sintering in air, is simple to operate, has low requirements on equipment and low generation cost, and the prepared fluorescence temperature measuring material has stable mechanical property and chemical property;
(3) the standard colorimetric card temperature measurement technology provided by the invention realizes low-cost temperature detection and provides a new application technology for an optical thermometer.
Drawings
FIG. 1 shows a single doping of 0.01Bi3+Excitation and emission spectra of (a);
FIG. 2 shows doping of Bi in different molar contents3+A comparison spectrum of the emission spectrum of (1);
FIG. 3 shows that 0.005Eu is singly doped3+Excitation and emission spectra of (a);
FIG. 4 shows the co-doping of Bi3+And Eu3+Excitation and emission spectra of (a);
FIG. 5 is a schematic diagram of the luminescence of the fluorescent thermometric material of the present invention;
FIG. 6 shows the fluorescence temperature measuring material (YNbO) prepared in example 14：0.01Bi3+-0.005Eu3+) X-ray diffraction patterns of (a);
FIG. 7 shows the fluorescence temperature measuring material (YNbO) prepared in example 14：0.01Bi3+-0.005Eu3+) A performance stability map of (a);
FIG. 8 shows the fluorescence temperature measuring material (YNbO) prepared in example 14：0.01Bi3+-0.005Eu3+) Emission spectra under the excitation of 318nm ultraviolet light and at different temperatures;
FIG. 9 shows the fluorescence temperature measuring material (YNbO) prepared in example 14：0.01Bi3+-0.005Eu3+) Middle Bi3+With Eu3+Intensity of ion emissionNormalized contrast map of (a);
FIG. 10 shows the fluorescence temperature measuring material (YNbO) prepared in example 14：0.01Bi3+-0.005Eu3+) A CIE coordinate diagram at different temperatures;
FIG. 11 shows the fluorescence temperature measuring material (YNbO) prepared in example 14：0.01Bi3+-0.005Eu3+) Color change profile with increasing temperature (camera shot);
FIG. 12 shows the fluorescence temperature measuring material (YNbO) prepared in example 14：0.01Bi3+-0.005Eu3+) As a function of 1/T;
FIG. 13 shows the fluorescence temperature measuring material (YNbO) prepared in example 14：0.01Bi3+-0.005Eu3+) Graph of Sa and Sr of (1) as a function of temperature;
FIG. 14 is a graph showing the temperature measurement of a glass sheet using the fluorescent thermometric material of the present invention;
FIG. 15 is a test chart of the fluorescent thermometric material of the present invention applied to measure water temperature.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be further described with reference to the accompanying drawings and examples.
The invention provides a thermochromic fluorescent temperature measuring material, which is Bi3+-Eu3+Codoping YNbO4The chemical formula is YNbO4：x Bi3+-y Eu3+Wherein x is more than or equal to 0.005 and less than or equal to 0.02; y is more than or equal to 0.002 and less than or equal to 0.03, and x represents Bi3+Substituted Y3+The molar content of (a); y represents Eu3+Substituted Y3+And x: y is in the range of 0.25 to 6. The substrate YNbO of the fluorescence temperature measuring material4The crystal structure is monoclinic system and transition metal ions Bi3+And rare earth ion Eu3+Combine to form two independent luminescent centers, wherein Bi3+Is a sensitizer, Eu3+Is an activator, and Bi is activated by ultraviolet light3+Ion generation of blue light emission and Eu3+The ions can generate stronger fluorescent radiation in the red light regionAnd is Bi3+To Eu3+The energy transfer efficiency of (2) is high.
YNbO as shown in FIG. 14:0.01Bi3+When monitored at 457nm, the fluorescence thermometric material emits a broadband excitation spectrum centered at 318nm, corresponding to1S0—3P1Transition; under 318nm excitation, the phosphor emits blue-violet light with a broad band centered at 457 nm.
As shown in FIG. 2, when Bi with different contents is doped3+The luminescence peak position of the fluorescence temperature measuring material is not changed, and only the luminescence intensity is influenced when the Bi is doped3+Has the maximum luminous intensity when the content of (1) is 0.01.
Eu single doping as shown in figure 33+The excitation spectrum has two broadband excitations between 240nm and 340nm, corresponding to O2-—Eu3+And sharp excitation peaks at 395nm,466nm and the like are 4f characteristic transitions. Under the excitation of 395nm, the fluorescent temperature measuring material emits obvious sharp peaks respectively corresponding to5D0-7FJ(J＝0,1,2,3,4)。
As shown in FIG. 4, we can see that Bi is singly doped3+Emission peak of ion and single doped Eu3+The excitation peaks of the ions have overlapping, indicating that Bi3+-Eu3+There may be energy transfer between them. Bi3+-Eu3+The emission and excitation diagram of the co-doped fluorescent thermometric material shows that: the excitation spectrum has obviously different broadband excitation at 250nm-350nm, mainly due to charge transfer band and1S0—3P1the transition is overlapped, and the emission spectrum has the characteristics of two emission centers, which are expressed as Bi3+Ion(s)3P1-1S0Blue-violet emission and Eu3+Characteristic red emission.
As shown in FIG. 5, the luminescence principle of the fluorescence temperature measuring material of the present invention is: fluorescent thermometric material (YNbO)4：x Bi3+-y Eu3+) Of Bi3+Under the excitation of ultraviolet rays with the wavelength of 318nm, electrons are removed from1S0Transition of ground state to1P1The excited state is transited to the lowest energy excited state through non-radiation, one part of electrons return to the ground state to emit 457nm broadband emission, and the other part of electrons are transferred to Eu through energy transfer3+Is/are as follows5D4The energy level is as low as 596nm, 614nm, 658nm and 706 nm. Benefit from Bi3+→Eu3+The fluorescent material can generate transition metal ions Bi under the effective excitation within the range of 250-350nm3+Blue-violet light and rare earth ion Eu3+Red light of (2).
YNbO is utilized as the fluorescent temperature measuring material4As doping ions Bi3+-Eu3+Substrate of (1), Compound YNbO prepared4：x Bi3+-y Eu3+High purity, good optical performance and stable physicochemical property, solves the problem of low sensitivity of a single luminescence center, and introduces Bi into the same matrix in the form of a combined pair of transition metal and rare earth ion3+-Eu3+The fluorescent temperature measuring material with the relative sensitivity of 1.63% is developed by utilizing the different luminescent colors and temperature quenching characteristics of the two luminescent centers, and theoretical guidance is provided for the fluorescent temperature measuring material based on the transition metal-rare earth ion type combination. Under the excitation of ultraviolet light, the phenomenon that the fluorescence temperature measuring material changes from purple to pink and finally to red can be seen by naked eyes within 473K (200 ℃), and the obvious color change enables people to directly observe the color change through naked eyes to measure the temperature.
The fluorescent temperature measuring material is prepared by a common high-temperature solid-phase synthesis method, and the temperature is too low to be beneficial to a substrate YNbO4The synthesis of single phase is easy to generate impurity phase, which affects the luminous intensity and has great influence on the thermochromism phenomenon; too high a temperature can cause serious agglomeration of the fluorescent thermometric material and produce a glassy phase, making it difficult to take the sintered fluorescent thermometric material out of the crucible, and furtherGrinding into powder. In order to effectively control production and obtain a fluorescent temperature measuring material with high sensitivity, in this embodiment, the sintering temperature may be 1250 to 1400 ℃, and the sintering time may be 3 to 5 hours.
The present invention provides a thermochromic fluorescent temperature measuring material, and a preparation method and applications thereof, which are described in detail below with reference to examples.
Example 1:
according to the general formula YNbO4:0.01Bi3+-0.005Eu3+The stoichiometric ratio of each element in the raw materials is that Y with the purity of more than 99 percent is accurately weighed2O3、Nb2O5、Bi2O3、Eu2O30.4497g Y2O3、0.5374g Nb2O5、0.0094g Bi2O3、0.0036g Eu2O3Mixing the materials in an agate mortar, adding alcohol to wet-grind for 30min until the sample is dried, then putting the sample into a high-temperature tube, sintering at 1300 ℃ for 4 hours, taking out the sample after the sample is cooled to room temperature, putting the sample into the mortar again, and dry-grinding the sample to powder to obtain the fluorescent temperature measuring material.
As shown in FIG. 6, the fluorescent thermometric material (YNbO) prepared in this example4：0.01 Bi3+-0.005 Eu3+) Middle Bi3+And Eu3+The doping does not change the structure of the fluorescence temperature measuring material and effectively enters YNbO4Y of the host lattice3+The lattice site of (1).
As shown in FIG. 7, the fluorescent thermometric material (YNbO) prepared in this example4：0.01 Bi3+-0.005 Eu3+) The fluorescent temperature measuring material has good optical performance and stable physical and chemical performance, and can keep good consistency after five times of heating cycles (298K-473K).
Testing fluorescent thermometric material YNbO4：0.01 Bi3+，0.005 Eu3+Spectral characteristics in the 298-475k temperature interval:
as shown in FIG. 8, the fluorescent thermometric material (YNbO 4: 0.01 Bi)3+-0.005Eu3+) Excited by 318nm ultraviolet lightEmission spectrum at the same temperature. The emission spectrum changes significantly with increasing temperature, as shown in FIG. 9, which shows Bi3+Emission intensity of is significantly reduced, and Eu3+The emission intensity of (2) decreases slowly. The corresponding color change is shown in FIG. 10, transitioning from blue to red in the CIE coordinates, and the fluorescent thermometric material (YNbO) was photographed by the cell phone4：0.01 Bi3+-0.005 Eu3+) The color at different temperatures also transitions from bluish purple to red as shown in fig. 11.
Thus, the fluorescence thermometric material (YNbO) can be seen4：0.01 Bi3+-0.005 Eu3+) The fluorescent temperature measuring material has a good thermochromism phenomenon, shows different colors after being excited by ultraviolet rays at different temperatures, and can realize a visual colorimetry temperature measuring technology according to the characteristic. Of course, the relative sensitivity and absolute sensitivity of the fluorescence thermometry material can also be measured according to the Fluorescence Intensity Ratio (FIR) technique. As shown in FIG. 12, by Eu3+Emission intensity at 614nm with Bi3+The emission intensity ratio at 457nm is plotted with the reciprocal of the temperature, a formula specific expression is fitted according to an exponential formula 1, and the fluorescence temperature measuring material (YNbO) is respectively calculated through formulas 2 and 34：0.01 Bi3+-0.005 Eu3+) The absolute sensitivity and the relative sensitivity of (a), the values of which are shown in fig. 13.
Equation 1: FIR ≈ B + Cexp (- Δ E/K)B T)
Equation 2:
equation 3:
the result shows that the fluorescence temperature measuring material prepared in the embodiment has the maximum sensitivity of 1.63% at 423K. And under the excitation of 318nm ultraviolet rays, the fluorescent temperature measuring material emits the change from blue light to red light.
The fluorescent thermometric material prepared in example 1 was applied to a standard colorimetric card thermometry technique. And comparing the color change of the fluorescent temperature measuring material with the color comparison area of the standard color comparison card to judge the temperature of the sample to be measured.
1. Temperature test for measuring glass Using fluorescent thermometric Material prepared in example 1
Placing the glass sheet on a temperature control heating table, then spreading the fluorescent temperature measuring material on the glass sheet, irradiating by an ultraviolet lamp with a wavelength of 318nm, wherein the color change of the fluorescent temperature measuring material is shown in figure 14 along with the rise of the temperature, and comparing with a standard color comparison card to obtain the temperature of the glass sheet.
2. The temperature test of measuring water was performed using the fluorescent thermometric material prepared in example 1.
Pouring the fluorescence temperature measuring material into water, mixing with water uniformly, placing on a temperature control heating table, irradiating with a 318nm ultraviolet lamp, changing the color of the fluorescence temperature measuring material with the temperature rise as shown in figure 15, and comparing with a standard color comparison card to obtain the water temperature.
Comparative example 1:
according to the general formula YNbO4：0.01 Bi3+-0.001 Eu3+The stoichiometric ratio of each element in the raw materials is that Y with the purity of more than 99 percent is accurately weighed2O3、Nb2O5、Bi2O3、Eu2O30.4468g Y2O3、0.5367g Nb2O5、0.0094g Bi2O3、0.0071g Eu2O3Mixing the materials in an agate mortar, adding alcohol to wet-grind for 30min until the sample is dried, then putting the sample into a high-temperature tube, sintering at 1300 ℃ for 4 hours, taking out the sample after the sample is cooled to room temperature, putting the sample into the mortar again, and dry-grinding the sample to powder to obtain the fluorescent temperature measuring material.
The fluorescent thermometric material (YNbO) of this comparative example was obtained according to the method of measuring the sensitivity of the fluorescent thermometric material according to the fluorescence intensity ratio technique (FIR) in example 14：0.01 Bi3+-0.001 Eu3+) The sensitivity was 1.51% maximal at 398K. And under the excitation of ultraviolet rays, fluorescent thermometric material (YNbO)4:0.01 Bi3+-0.001 Eu3+) Is emitted fromPurple to red light.
In summary, by comparing example 1 with comparative example 1, we can find out to control Bi3+Increase Eu while keeping the doping content constant3+The relative sensitivity is rather lowered, which indicates that Eu must be controlled to obtain a higher sensitivity3+Must not be too much because of Bi3+-Eu3+There is an energy transfer between, Eu3+The increase of the content results in Bi3+Resulting in an increase in the range of FIR values and thus in a decrease in relative sensitivity.
The temperature measuring method of the invention is based on Bi3+With Eu3+The emission intensity of the ions has a tendency to decay with temperature. When Eu is used3+When the ion content is too large, Bi is caused3+The emission intensity of (A) becomes small, thereby the Bi of the fluorescence thermometric material becomes small3+The degree of attenuation of the blue emission becomes smaller with the temperature change, which is not favorable for the improvement of the relative sensitivity. And Eu3+The increase in the content results in Bi3+The blue emission is greatly reduced, so that the red light of the temperature measuring material is much under the excitation of ultraviolet light at normal temperature, the blue light is less, and the thermochromic phenomenon of the temperature measuring material is not facilitated. Therefore, the difference of the luminescent colors of the fluorescent temperature measuring materials along with the temperature change is reduced, and the observation by naked eyes is not facilitated. Thus, fluorescent thermometric material (YNbO)4:0.01 Bi3+，0.005 Eu3+) Under 318nm ultraviolet laser, the change from blue light to red light is emitted along with the temperature change, and within 473K (200 ℃), an obvious color change phenomenon can be observed by naked eyes, namely, the blue-violet color is changed into pink color and finally the red color is changed.
The features of the embodiments and embodiments described herein above may be combined with each other without conflict.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. A thermochromic fluorescent temperature measurement material is characterized in that: the fluorescent temperature measuring material is Bi3+-Eu3+Doping YNbO4The chemical formula is YNbO4：x Bi3+-y Eu3+Wherein x is more than or equal to 0.005 and less than or equal to 0.02; y is more than or equal to 0.002 and less than or equal to 0.03, and x represents Bi3+Substituted Y3+The molar content of (a); y represents Eu3+Substituted Y3+The molar content of (a).
2. The thermochromic fluorescent thermometric material of claim 1, wherein: the ratio x to y of x to y is in the range of 0.25-6.
3. A method of preparing the thermochromic fluorescent thermometric material of claim 1, wherein: the method comprises the following steps:
s1 according to the chemical formula YNbO4：x Bi3+-y Eu3+Weighing solid compounds containing Y, Nb, Bi and Eu elements according to the stoichiometric ratio of the elements, and putting the solid compounds into a mortar for uniform grinding to obtain a mixture;
s2, placing the mixture into a high-temperature tube furnace, and sintering for 2-6 hours at the temperature of 1200-1500 ℃ in an air environment;
and S3, taking the mixture out of the tube furnace after the mixture is cooled, and grinding the mixture into powder again to obtain the fluorescent temperature measuring material.
4. The method of claim 3, wherein the thermochromic fluorescent thermometric material is prepared by: in step S1, the solid compound is one or more of oxides, carbonates, or nitrates containing Y, Nb, Bi, and Eu elements.
5. The method of claim 3, wherein the thermochromic fluorescent thermometric material is prepared by: in the step S2, the sintering temperature is 1250-1400 ℃.
6. The method of claim 5, wherein the thermochromic fluorescent thermometric material is prepared by: the sintering time is 3-5 hours.
7. Use of the thermochromic fluorescent thermometric material of claim 1, wherein: the fluorescent temperature measuring material is applied to a standard colorimetric card temperature measuring technology.
8. The use of a thermochromic fluorescent thermometric material according to claim 7, wherein: the temperature measuring range of the standard colorimetric card temperature measuring technology is 298K-473K.
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| CN114702946A (en) * | 2022-04-11 | 2022-07-05 | 成都大学 | Thermoluminescent color-changing temperature-measuring fluorescent material and preparation method thereof |
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| JIANG ZIQIANG: "Design, luminescence and energy transfer of single-phased color-tunable YNbO4:Bi3+, Eu3+ phosphor for UV pumped white light-emitting diodes", 《JOURNAL OF MATERIALS SCIENCE-MATERIALS IN ELECTRONICS》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114702946A (en) * | 2022-04-11 | 2022-07-05 | 成都大学 | Thermoluminescent color-changing temperature-measuring fluorescent material and preparation method thereof |
| CN114702946B (en) * | 2022-04-11 | 2024-01-26 | 成都大学 | Thermoluminescent color-changing temperature-measuring fluorescent material and preparation method thereof |
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